CN103361533B - Titanium carbide-based solid solution metal ceramic and preparation method thereof - Google Patents
Titanium carbide-based solid solution metal ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses titanium carbide-based solid solution metal ceramic and a preparation method thereof. The titanium carbide-based solid solution metal ceramic is composed of a hard phase (Ti, W) C solid solution and an adhesive phase Ni, wherein the composite material powder is prepared by mold pressing forming, degreasing and vacuum sintering; the composite material is synthesized by utilizing Ti powder, W powder, Ni powder and graphite powder as raw materials and performing a high-energy ball milling induced self-propagating reaction under argon protection, and the raw materials comprise the following ingredient by mass percent: 40.60-58.02% of Ti powder, 11.02-29.18% of W powder, 15.00-20.00% of Ni powder and 11.94-15.27% of graphite powder. The preparation of solid solution powder is simple in process, short in cycle, low in energy consumption and easy to control the oxygen content, the hardness of the prepared titanium carbide-based solid solution metal ceramic is 89.0-91.8HRA, the bending strength is not smaller than 1680MPa, and the fracture toughness KIC is not smaller than 12.5MPa.m1/2, so that the titanium carbide-based solid solution metal ceramic is suitable for serving as high-speed and high-efficiency cutting tools, hot extrusion molds and heat-resistant, corrosion-resistant and wear-resistant parts and components.
Description
Technical field
The invention belongs to cermet material and powder metallurgical technology, be specifically related to a kind of titanium carbide base solid solution cermet(SSC) and preparation method thereof.
Background technology
TiC or Ti (C, N) based ceramic metal are that a kind of TiC of take or Ti (C, N) are as main hard phase, Ni or Co or (Ni+Co) Binder Phase, the Particle reinforced composite that adopts powder metallurgical technique to prepare.Compare with WC-Co Wimet, sintering metal has more excellent high temperature red hardness, wear resistance and oxidation-resistance, and it and intermetallic frictional coefficient are lower, it is the ideal material of making high-speed and high-efficiency cutting tool, hot forming tool and the anti-corrosion component of heat-resistant antifriction.In addition, ceramic-metallic main raw material Ti reserves are abundant, and its cost of manufacture is only 35～55% of Wimet, therefore enjoy investigation of materials personnel's concern.Although by adding Mo
2the additives such as C (or Mo), WC can significantly improve the wettability between hard phase and Binder Phase, thereby have improved to a certain extent ceramic-metallic obdurability, but (fracture toughness property is 9～16MPam approximately with Wimet high tenacity
1/2) compare, the toughness of Ti (C, N) based ceramic metal is still lower, and (fracture toughness property is about 6～9MPam
1/2), in vibrations, easily there is brittle failure under compared with large Service Environment and lost efficacy, this also becomes the main factor that this material of restriction replaces WC-Co Wimet.
Traditional TiC or Ti (C, N) based ceramic metal are generally by adding Mo
2the Equations of The Second Kind carbide such as C (or Mo), WC and TaC (or NbC) improve ceramic-metallic sinterability, high temperature red hardness, heat-shock resistance and high temperature plasticity_resistant deformation ability.Adding of these additives makes ceramic-metallic microstructure present typical core-ring structure: core is undissolved TiC or Ti (C in sintering process mutually, N) particle, annular is (Ti mutually, M) C or (Ti, M) (C, N) sosoloid (M is the transition metals such as W, Mo, Ta, Nb, lower same).Wherein annular consists of inside and outside annular phase two portions again mutually: interior annular is mutually near core-ring interface, is rich in the heavy elements such as W, Mo and Ti constituent content is lower; Outer ring is mutually near annular phase-Binder Phase interface, is rich in Ti element and the contents of heavy metal elements such as W, Mo are lower.Although annular has been improved the wettability between ceramic crystalline grain and metallic binding phase mutually, but interior annular phase, outer ring phase and a large amount of phase interface of the alternate existence of core, and due to the difference in composition transitivity parameter, on these phase interfacies, produced complicated interfacial stress, when material is subject to external load function, crackle easily germinates and breeds on these interfaces.This is that the obdurability of Ti (C, N) based ceramic metal is lower than the one of the main reasons of Wimet.
Inspiration based on WC-Co Wimet two phase structure, TiC or Ti (C, N) base metal-ceramic material researchist is by Ti (C, N) hard phase in based ceramic metal and Equations of The Second Kind carbide additive are prepared polynary titanium carbide base or titanium carbonitride based solid solution by pre-solid solution, thereby realize the Ti (C of the double structure with similar WC-Co Wimet, N) base metal-ceramic material, has improved the obdurability of Ti (C, N) based ceramic metal.Current titanium carbide base or titanium carbonitride based solid solution powder are mainly by adopting carbothermic reduction oxide powder to prepare.The Chinese patent of publication number CN1854140A, adopts after high-energy ball milling oxide powder, then synthesizes (Ti, W) C and (Ti, W) (C, N) solid-solution powder by carbothermic reduction, and prepares based on this high-fracture toughness (11～13MPam
1/2) Ti (C, N) based ceramic metal; Carbothermic reduction is according to more than the composition high-energy ball milling 48h of design by the oxide compound of required solid solution element, then in more than 1300 ℃ vacuum oven (or atmosphere furnace), reduce mixed powder and obtain solid-solution powder, yet the method preparation cycle is long, energy consumption is large and oxygen level is wayward.
Summary of the invention
The invention provides a kind of titanium carbide base solid solution cermet(SSC), its preparation method is provided simultaneously, when solving existing carbothermic method and preparing titanium carbide base solid-solution powder, preparation cycle is long, energy consumption is large and the uppity problem of oxygen level.
A kind of titanium carbide base solid solution cermet(SSC) provided by the present invention, is comprised of hard phase (Ti, W) C sosoloid and Binder Phase Ni, it is characterized in that:
It is made through die forming, degreasing and vacuum sintering by compound material powder;
It is raw material that described compound material be take Ti powder, W powder, Ni powder and Graphite Powder 99; under argon shield, adopt high-energy ball milling to bring out self-propagating reaction synthetic; in raw material, the mass percent of each component is: Ti powder 40.60%～58.02%; W powder 11.02%～29.18%; Ni powder 15.00%～20.00%, Graphite Powder 99 11.94%～15.27%.
The preparation method of described titanium carbide base solid solution cermet(SSC), comprises the following steps successively:
(1) Ti powder, W powder, Ni powder and Graphite Powder 99 are dropped in ball grinder, and be filled with argon gas, on planetary ball mill, carry out high-energy ball milling, bring out self-propagating reaction, obtain (Ti, W) C-Ni compound material powder; The mass percent of each component is: Ti powder 40.60%～58.02%, W powder 11.02%～29.18%, Ni powder 15.00%～20.00%, Graphite Powder 99 11.94%～15.27%;
(2) resulting (Ti, W) C-Ni compound material powder is mixed to 2wt%～3wt% binder polyoxyethylene glycol (PEG), then die forming under 150MPa～300MPa pressure, makes pressed compact;
(3) pressed compact is carried out in vacuum oven to vacuum degreasing, vacuum tightness is higher than 5Pa, 250 ℃～450 ℃ of skimming temps, soaking time 8h～12h;
(4) to the pressed compact after degreasing higher than 1 * 10
-1under Pa vacuum tightness, carry out sintering, obtain titanium carbide base solid solution cermet(SSC), sintering temperature is 1440 ℃～1455 ℃, and soaking time is 45min～60min.
Described preparation method, it is further characterized in that: while carrying out described high-energy ball milling, ratio of grinding media to material is 25:1～30:1, rotating speed >=350rpm, Ball-milling Time 4h～6h.
The present invention utilizes Ti to react with C to generate the feature of the high heat release of TiC, adopts high-energy ball milling mode to light reacting between Ti and C under argon shield, and under self exothermic effects, reaction continues to carry out until finish (being self-propagating reaction); Under high reaction heat effect, W solid solution forms (Ti, W) C sosoloid in TiC.Not only the simple efficiency of technique is high for solid-solution powder preparation method of the present invention, and synthetic solid-solution powder granularity tiny, be evenly distributed and oxygen level low, the more important thing is, because making metal Ni fusing, the feature of the high thermal discharge of self-propagating reaction forms liquid phase, under liquid phase effect Ti and C react and the solid solution of W can be carried out quickly by diffusion, in process of cooling, (Ti, W) C separates out from liquid phase Ni.Synthetic (Ti, W) C sosoloid and the Ni of this original position has good interface bonding state, thereby makes hard phase and Binder Phase after sintering have higher interface bond strength.In addition, the machinery that the present invention adopts brings out Metal-ceramie powder powder stock phase composite prepared by self-propagating reaction and not only comprises (Ti, W) C solid solution phase and metal Ni, also has the not W of complete reaction.In ceramic-metallic sintering process, remain W and react generation WC with remaining graphite, thereby further improved the bonding strength of hard phase and Binder Phase.The microstructure of resulting titanium carbide base solid solution cermet(SSC) is comprised of centreless-ring structure and two kinds of ceramic crystalline grains of weak core-ring structure.
The present invention prepares that solid-solution powder technique is simple, the cycle is short, energy consumption is low and oxygen level is easy to control, prepared titanium carbide base solid solution cermet(SSC) hardness 89.0HRA～91.8HRA, bending strength>=1680MPa, fracture toughness property K
iC>=12.5MPam
1/2there is excellent shock resistance, wear resistance, high temperature red hardness, chemical stability and anti-adhesive, be suitable as high-speed and high-efficiency cutting tool (being especially applicable to the difficult-to-machine materials such as high-speed dry type cutting stainless steel, iron-base superalloy, High Strength Structural Steel, graphitic cast iron), hot-extrusion mold and heat-resistant anti-corrosion abrasion-proof component.
Accompanying drawing explanation
Fig. 1 is the X diffracting spectrum of the compound material powder prepared of the present invention, and in figure, θ is diffraction angle;
Fig. 2 is the X diffracting spectrum of the titanium carbide base solid solution cermet(SSC) prepared of the present invention, and in figure, θ is diffraction angle;
Fig. 3 is the stereoscan photograph of the titanium carbide base solid solution cermet(SSC) prepared of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1, comprises the following steps successively:
(1) Ti powder, W powder, Ni powder and Graphite Powder 99 are dropped in ball grinder, and be filled with argon gas, carry out high-energy ball milling on planetary ball mill, bring out self-propagating reaction, obtain (Ti, W) C-Ni compound material powder, its X diffracting spectrum is shown in Fig. 1; The mass percent of each component is: Ti powder 54.61%, W powder 11.02%, Ni powder 20.00%, Graphite Powder 99 14.37%;
Ti Powder Particle Size 45 μ m, purity 99%, W Powder Particle Size 3.80 μ m, purity 99.9%, Ni Powder Particle Size 2.25 μ m, purity 99.8%, Graphite Powder 99 granularity 5.5 μ m, purity 99.9%;
While carrying out high-energy ball milling, ratio of grinding media to material is 25:1, rotating speed 350rpm, Ball-milling Time 6h;
(2) resulting (Ti, W) C-Ni compound material powder is mixed to 3wt% binder polyoxyethylene glycol (PEG), then die forming under 150MPa pressure, makes pressed compact;
(3) pressed compact is carried out in vacuum oven to vacuum degreasing, vacuum tightness is 1Pa～5Pa, 450 ℃ of skimming temps, soaking time 8h;
(4) to the pressed compact after degreasing higher than 1 * 10
-2under Pa vacuum tightness, carry out sintering, obtain titanium carbide base solid solution cermet(SSC), sintering temperature is 1440 ℃, and soaking time is 45min; The prepared titanium carbide base solid solution cermet(SSC) performance of the present embodiment is in Table 1, and its X diffracting spectrum is shown in Fig. 2, and its stereoscan photograph is shown in Fig. 3.
Embodiment 2, comprise the following steps successively:
(1) Ti powder, W powder, Ni powder and Graphite Powder 99 are dropped in ball grinder, and be filled with argon gas, on planetary ball mill, carry out high-energy ball milling, bring out self-propagating reaction, obtain (Ti, W) C-Ni compound material powder; The mass percent of each component is: Ti powder 40.60%, W powder 27.46%, Ni powder 20.00%, Graphite Powder 99 11.94%;
Ti Powder Particle Size 45 μ m, purity 99%, W Powder Particle Size 3.80 μ m, purity 99.9%, Ni Powder Particle Size 2.25 μ m, purity 99.8%, Graphite Powder 99 granularity 5.5 μ m, purity 99.9%;
While carrying out high-energy ball milling, ratio of grinding media to material is 30:1, rotating speed 400rpm, Ball-milling Time 4h.
(2) resulting (Ti, W) C-Ni compound material powder is mixed to 3wt% binder polyoxyethylene glycol (PEG), then die forming under 200MPa pressure, makes pressed compact;
(3) pressed compact is carried out in vacuum oven to vacuum degreasing, vacuum tightness is higher than 1Pa～5Pa, 400 ℃ of skimming temps, soaking time 10h;
(4) to the pressed compact after degreasing higher than 1 * 10
-2under Pa vacuum tightness, carry out sintering, obtain titanium carbide base solid solution cermet(SSC), sintering temperature is 1440 ℃, and soaking time is 45min; The prepared titanium carbide base solid solution cermet(SSC) performance of the present embodiment is in Table 1.
Embodiment 3, comprise the following steps successively:
(1) Ti powder, W powder, Ni powder and Graphite Powder 99 are dropped in ball grinder, and be filled with argon gas, on planetary ball mill, carry out high-energy ball milling, bring out self-propagating reaction, obtain (Ti, W) C-Ni compound material powder; The mass percent of each component is: Ti powder 48.13%, W powder 20.50%, Ni powder 18.00%, Graphite Powder 99 13.37%;
Ti Powder Particle Size 45 μ m, purity 99%, W Powder Particle Size 3.80 μ m, purity 99.9%, Ni Powder Particle Size 2.25 μ m, purity 99.8%, Graphite Powder 99 granularity 5.5 μ m, purity 99.9%;
While carrying out high-energy ball milling, ratio of grinding media to material is 30:1, rotating speed 350rpm, Ball-milling Time 5h.
(2) resulting (Ti, W) C-Ni compound material powder is mixed to 2.5wt% binder polyoxyethylene glycol (PEG), then die forming under 250MPa pressure, makes pressed compact;
(3) pressed compact is carried out in vacuum oven to vacuum degreasing, vacuum tightness is higher than 1Pa～5Pa, 350 ℃ of skimming temps, soaking time 10h;
(4) to the pressed compact after degreasing higher than 1 * 10
-2under Pa vacuum tightness, carry out sintering, obtain titanium carbide base solid solution cermet(SSC), sintering temperature is 1455 ℃, and soaking time is 50min; The prepared titanium carbide base solid solution cermet(SSC) performance of the present embodiment is in Table 1.
Embodiment 4, comprise the following steps successively:
(1) Ti powder, W powder, Ni powder and Graphite Powder 99 are dropped in ball grinder, and be filled with argon gas, on planetary ball mill, carry out high-energy ball milling, bring out self-propagating reaction, obtain (Ti, W) C-Ni compound material powder; The mass percent of each component is: Ti powder 49.30%, W powder 21.00%, Ni powder 16.00%, Graphite Powder 99 13.70%;
Ti Powder Particle Size 45 μ m, purity 99%, W Powder Particle Size 3.80 μ m, purity 99.9%, Ni Powder Particle Size 2.25 μ m, purity 99.8%, Graphite Powder 99 granularity 5.5 μ m, purity 99.9%;
While carrying out high-energy ball milling, ratio of grinding media to material is 25:1, rotating speed 400rpm, Ball-milling Time 5h.
(2) resulting (Ti, W) C-Ni compound material powder is mixed to 2.5wt% binder polyoxyethylene glycol (PEG), then die forming under 300MPa pressure, makes pressed compact;
(3) pressed compact is carried out in vacuum oven to vacuum degreasing, vacuum tightness is higher than 1Pa～5Pa, 350 ℃ of skimming temps, soaking time 10h;
(4) to the pressed compact after degreasing higher than 1 * 10
-1under Pa vacuum tightness, carry out sintering, obtain titanium carbide base solid solution cermet(SSC), sintering temperature is 1452 ℃, and soaking time is 55min; The prepared titanium carbide base solid solution cermet(SSC) performance of the present embodiment is in Table 1.
Embodiment 5, comprise the following steps successively:
(1) Ti powder, W powder, Ni powder and Graphite Powder 99 are dropped in ball grinder, and be filled with argon gas, on planetary ball mill, carry out high-energy ball milling, bring out self-propagating reaction, obtain (Ti, W) C-Ni compound material powder; The mass percent of each component is: Ti powder 58.02%, W powder 11.71%, Ni powder 15.00%, Graphite Powder 99 15.27%;
Ti Powder Particle Size 45 μ m, purity 99%, W Powder Particle Size 3.80 μ m, purity 99.9%, Ni Powder Particle Size 2.25 μ m, purity 99.8%, Graphite Powder 99 granularity 5.5 μ m, purity 99.9%;
While carrying out high-energy ball milling, ratio of grinding media to material is 25:1, rotating speed 350rpm, Ball-milling Time 6h.
(2) resulting (Ti, W) C-Ni compound material powder is mixed to 2wt% binder polyoxyethylene glycol (PEG), then die forming under 300MPa pressure, makes pressed compact;
(3) pressed compact is carried out in vacuum oven to vacuum degreasing, vacuum tightness is higher than 1Pa～5Pa, 250 ℃ of skimming temps, soaking time 12h;
(4) to the pressed compact after degreasing higher than 1 * 10
-1under Pa vacuum tightness, carry out sintering, obtain titanium carbide base solid solution cermet(SSC), sintering temperature is 1455 ℃, and soaking time is 60min; The prepared titanium carbide base solid solution cermet(SSC) performance of the present embodiment is in Table 1.
Embodiment 6, comprise the following steps successively:
(1) Ti powder, W powder, Ni powder and Graphite Powder 99 are dropped in ball grinder, and be filled with argon gas, on planetary ball mill, carry out high-energy ball milling, bring out self-propagating reaction, obtain (Ti, W) C-Ni compound material powder; The mass percent of each component is: Ti powder 43.13%, W powder 29.18%, Ni powder 15.00%, Graphite Powder 99 12.69%;
Ti Powder Particle Size 45 μ m, purity 99%, W Powder Particle Size 3.80 μ m, purity 99.9%, Ni Powder Particle Size 2.25 μ m, purity 99.8%, Graphite Powder 99 granularity 5.5 μ m, purity 99.9%;
While carrying out high-energy ball milling, ratio of grinding media to material is 30:1, rotating speed 400rpm, Ball-milling Time 4h.
(2) resulting (Ti, W) C-Ni compound material powder is mixed to 2wt% binder polyoxyethylene glycol (PEG), then die forming under 300MPa pressure, makes pressed compact;
(3) pressed compact is carried out in vacuum oven to vacuum degreasing, vacuum tightness is higher than 1Pa～5Pa, 300 ℃ of skimming temps, soaking time 12h;
(4) to the pressed compact after degreasing higher than 1 * 10
-1under Pa vacuum tightness, carry out sintering, obtain titanium carbide base solid solution cermet(SSC), sintering temperature is 1455 ℃, and soaking time is 60min; The prepared titanium carbide base solid solution cermet(SSC) performance of the present embodiment is in Table 1.
The mechanical property of table 1 titanium carbide base solid solution cermet(SSC)
Claims (3)
1. a titanium carbide base solid solution cermet(SSC), is comprised of hard phase (Ti, W) C sosoloid and Binder Phase Ni, it is characterized in that:
It is made through die forming, degreasing and vacuum sintering by compound material powder;
It is raw material that described compound material be take Ti powder, W powder, Ni powder and Graphite Powder 99; under argon shield, adopt high-energy ball milling to bring out self-propagating reaction synthetic; in raw material, the mass percent of each component is: Ti powder 40.60%～58.02%; W powder 11.02%～29.18%; Ni powder 15.00%～20.00%, Graphite Powder 99 11.94%～15.27%.
2. the preparation method of titanium carbide base solid solution cermet(SSC) as claimed in claim 1, comprises the following steps successively:
(1) Ti powder, W powder, Ni powder and Graphite Powder 99 are dropped in ball grinder, and be filled with argon gas, on planetary ball mill, carry out high-energy ball milling, bring out self-propagating reaction, obtain (Ti, W) C-Ni compound material powder; The mass percent of each component is: Ti powder 40.60%～58.02%, W powder 11.02%～29.18%, Ni powder 15.00%～20.00%, Graphite Powder 99 11.94%～15.27%;
(2) resulting (Ti, W) C-Ni compound material powder is mixed to 2wt%～3wt% binder polyoxyethylene glycol, then die forming under 150MPa～300MPa pressure, makes pressed compact;
(3) pressed compact is carried out in vacuum oven to vacuum degreasing, vacuum tightness is higher than 5Pa, 250 ℃～450 ℃ of skimming temps, soaking time 8h～12h;
(4) to the pressed compact after degreasing higher than 1 * 10
-1under Pa vacuum tightness, carry out sintering, obtain titanium carbide base solid solution cermet(SSC), sintering temperature is 1440 ℃～1455 ℃, and soaking time is 45min～60min.
3. preparation method as claimed in claim 2, is characterized in that: while carrying out described high-energy ball milling, ratio of grinding media to material is 25:1～30:1, rotating speed >=350rpm, Ball-milling Time 4h～6h.
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| CN104911426A (en) * | 2015-06-25 | 2015-09-16 | 西安交通大学 | Preparation method of AlN particle enhanced Mg-Al based composite material |
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